CN110054855B - Polytetrafluoroethylene bubble point membrane and preparation method thereof - Google Patents
Polytetrafluoroethylene bubble point membrane and preparation method thereof Download PDFInfo
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- CN110054855B CN110054855B CN201910120130.1A CN201910120130A CN110054855B CN 110054855 B CN110054855 B CN 110054855B CN 201910120130 A CN201910120130 A CN 201910120130A CN 110054855 B CN110054855 B CN 110054855B
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- polytetrafluoroethylene
- bubble point
- heat setting
- polytetrafluoroethylene resin
- stretching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
- B29C55/143—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly parallel to the direction of feed and then transversely thereto
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
Abstract
The invention relates to the technical field of thin films, in particular to a polytetrafluoroethylene bubble point film and a preparation method thereof, wherein the polytetrafluoroethylene bubble point film is prepared from polytetrafluoroethylene resin with the molecular weight of 105‑107And the molecular weight of the polytetrafluoroethylene resin a is 107‑108The particle diameter ratio of the polytetrafluoroethylene resin a to the polytetrafluoroethylene resin b is 95-105: 100, the preparation method comprises a heat setting step after biaxial stretching, wherein the heat setting temperature is 320-340 ℃, and the heat setting time is 30-60 s. The bubble point membrane obtained by the invention has the advantages of about 0.2 micron pore diameter, uniform pore diameter distribution and high stability.
Description
Technical Field
The invention relates to the technical field of films, in particular to a polytetrafluoroethylene bubble point film and a preparation method thereof.
Background
The Polytetrafluoroethylene (PTFE) film has the disadvantages of complex manufacturing method, long working procedure and many influencing factors, so that the problems of high-quality products to be produced in large scale are high, the low-molecular-weight PTFE has low strength and small tensile aperture ratio, and the high-molecular-weight polymer has good strength and high porosity. However, the perfluorinated linear high molecular weight polymer has large particles, high melting point and high melt viscosity, and the film production method thereof is an unconventional process. Patent CN1193060A proposes that the effect of expansion setting is better when the temperature is 1000-1500 ℃, and it is considered that the high-temperature setting is more than ten times, the strength of the membrane is high, and the aperture is stable, but the method of ultra-high temperature expansion setting is difficult to control in production practice.
PTFE bubble point membranes are generally made from Polytetrafluoroethylene (PTFE) suspension powder. The membrane is prepared by adopting a unique biaxial tension technology, can ensure that impurities such as bacteria and the like are completely intercepted, and has larger flux, wherein the size and the uniform distribution of the membrane pore diameter are important, and when the membrane pore diameter is smaller and the distribution is more uniform, the bubble point value of the membrane is higher, and the interception effect is better. The patent with the application number of CN201410149632 provides a preparation method of a polytetrafluoroethylene bubble point film, and a bubble point film with the pore diameter of 0.4-0.5 micrometer is obtained by mixing polytetrafluoroethylene resin and polystyrene resin, so that the degerming effect cannot be met, and the pore diameter of a common bubble point film which can play a degerming effect is 0.2 micrometer.
Disclosure of Invention
Aiming at the problems, the invention provides a polytetrafluoroethylene bubble point membrane and a preparation method thereof, wherein the polytetrafluoroethylene bubble point membrane with the pore size of about 0.2 micron, uniform distribution and high stability is obtained by reasonably screening raw materials of tetrafluoroethylene resin and selecting proper proportion and particle size of polytetrafluoroethylene resin with different molecular weights.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a polytetrafluoroethylene bubble point membrane is prepared from polytetrafluoroethylene resin with molecular weight of 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The particle diameter ratio of the polytetrafluoroethylene resin a to the polytetrafluoroethylene resin b is 95-105: 100.
generally, the pore diameter of the bubble point membrane is about 0.2 micron, so that an ideal sterilization effect can be achieved, the pore diameter of the bubble point membrane obtained by taking single polytetrafluoroethylene resin as a raw material cannot reach 0.2 micron, other resins are often required to be added, but the single polytetrafluoroethylene resin is a high-temperature melting process in a shaping process, the single polytetrafluoroethylene resin is a polymer with uneven molecular weight, the melting points of the polytetrafluoroethylene resins with different molecular weights have fluctuation intervals, after the other resins are added, the melting temperature is difficult to control, all the polytetrafluoroethylene resins are easy to melt, the pore-forming performance of the polytetrafluoroethylene self-mechanical structure is damaged, the instability of the pore diameter is further caused, and the pore diameter is too large or the uniformity is poor. The raw materials are reasonably controlled, the polytetrafluoroethylene resin b with larger overall molecular weight is taken as a main material, the polytetrafluoroethylene resin a with smaller overall molecular weight is taken as an auxiliary material, the particle size of all the polytetrafluoroethylene resins fluctuates within the range of +/-5% of the average particle size of the polytetrafluoroethylene resin b, and the melting point of the polytetrafluoroethylene resin b with larger melting point of the polytetrafluoroethylene resin a with smaller molecular weight is lower, so that the polytetrafluoroethylene resin a with smaller molecular weight can fill the solid polytetrafluoroethylene resin b with larger molecular weight when being melted, and further the bubble point membrane with small pore diameter and uniform micropore distribution is obtained. The particle size of the raw materials directly influences the aperture and the aperture stability of the bubble point membrane of the product, and the resin with similar aperture has better conformity in a molten state.
Preferably, the weight ratio of the polytetrafluoroethylene resin a to the polytetrafluoroethylene resin b is (1-6): 20, the molecular weight of the polytetrafluoroethylene resin a is small, and the pore diameter of the polytetrafluoroethylene resin b is filled after melting, so the amount is not suitable to be too large, otherwise, the bubble point membrane pores are easy to be blocked.
Preferably, the bubble point membrane has a pore size of 0.1 to 0.3 micron and a porosity of 85 to 95%.
A preparation method of a polytetrafluoroethylene bubble point membrane comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxial stretching, and also comprises a heat setting step after biaxial stretching, wherein the heat setting temperature in the heat setting step is 320-340 ℃, and the heat setting time is 30-60 s.
Further preferably, the mixing temperature is 10-20 ℃; the curing temperature is 60-90 ℃.
Preferably, the cooling rate of the heat setting is 20-70 ℃/min, the heat setting is favorable for stabilizing the structural molding of the bubble point film, the reasonable control of the cooling rate is favorable for improving the toughness of the strength of the bubble point film, and the excessive cooling rate easily causes internal stress inside the bubble point film to damage the uniformity of the bubble point film.
Preferably, the biaxial stretching process comprises longitudinal stretching with stretching ratio of 3-10 times and transverse stretching with stretching ratio of 5-12 times, which is favorable for the tensile strength of the bubble point film.
Preferably, a double-cone mixer is adopted for mixing during mixing, the double-cone mixer rotates clockwise for 10-30min and rotates anticlockwise for 10-30min after standing for 0-5min, and polytetrafluoroethylene resins with different molecular weights are mixed by collision ceaselessly when the double-cone mixer is adopted for mixing, so that the mixing uniformity is improved. When the double-cone mixer rotates for mixing, the heat production is large, and the structural change of the polytetrafluoroethylene resin is easily caused, so that the continuous mixing time is controlled, the polytetrafluoroethylene resin is reversely mixed after being placed for about 3min in a static way, and the situation that the polytetrafluoroethylene resin with different molecular weights (different in quality and different in inertia) is layered in the mixer to influence the mixing effect is avoided.
According to the invention, the polytetrafluoroethylene bubble point membrane with fine pore diameter, uniform pore diameter distribution and good pore diameter stability is obtained by controlling the material mixing process and the heat setting process in the preparation process of the bubble point membrane. In the material mixing process, firstly, polytetrafluoroethylene raw materials with similar particle sizes are screened out, the weight ratio of polytetrafluoroethylene resins with different molecular weights is reasonably controlled to achieve the uniformity of the aperture of a subsequent bubble point film, a double-cone mixer is utilized to reasonably control the mixing temperature and time, the conventional process operation is carried out after an auxiliary agent is added, after the bidirectional stretching, the thermal setting operation is adopted, the polytetrafluoroethylene resin is a polymer with multiple molecular weights, the melting point of the polytetrafluoroethylene resin is 327 ℃, the thermal setting temperature is controlled to be 340 ℃, in the temperature environment, the polytetrafluoroethylene resin a with small molecular weight is changed into a molten state due to the lower melting point, the polytetrafluoroethylene resin b with large molecular weight is not changed in shape due to the relatively higher melting point, the original mechanical structure of the polytetrafluoroethylene resin is kept, after the thermal setting, the bubble point membrane is not easy to shrink and deform, and the aperture stability is greatly improved.
The invention has the following advantages:
(1) the pore diameter of the polytetrafluoroethylene bubble point membrane obtained by the invention is about 0.2 micron, the polytetrafluoroethylene bubble point membrane has excellent degerming performance, the pore diameters are normally distributed, the pore diameter distribution is uniform, and the stability is high.
(2) According to the invention, a physical blending method in a double-cone mixer is adopted in the mixing process, the stirring is soft, and the condition that the thermoplastic resin structure is damaged due to overhigh temperature and overhigh stirring strength in the mixing process is avoided.
(3) According to the invention, through reasonably controlling the heat setting process, the low molecular weight polytetrafluoroethylene resin is melted, and the high molecular weight polytetrafluoroethylene resin keeps the original mechanical form, so that the problems of shrinkage deformation and the like of the formed bubble point membrane are avoided, and the stability of the aperture is kept.
Detailed Description
The present embodiments are to be considered in all respects as illustrative and not restrictive. Any changes that may be made by one of ordinary skill in the art after reading the specification herein are, within the purview of the appended claims, to fall within the scope of the patent laws.
Raw material 1:
molecular weight is 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The weight ratio of the polytetrafluoroethylene resin b is 1: 20, average particle diameter ratio of 95: 100.
raw material 2:
molecular weight is 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The weight ratio of the polytetrafluoroethylene resin b is 6: 20, average particle diameter ratio of 105: 100.
raw material 3:
molecular weight is 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The weight ratio of the polytetrafluoroethylene resin b is 3: 20, average particle diameter ratio of 100: 100.
raw material 4:
molecular weight is 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The weight ratio of the polytetrafluoroethylene resin b is 1: 20, average particle diameter ratio of 100: 100.
raw material 5:
molecular weight is 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The weight ratio of the polytetrafluoroethylene resin b is 5: 20, average particle diameter ratio of 95: 100.
example 1:
a preparation method of polytetrafluoroethylene comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxially stretching, and further comprising a step of heat setting after biaxially stretching, wherein the heat setting temperature is 320 ℃, the heat setting time is 30s, and the cooling rate of the heat setting is 20 ℃/min; wherein, the material mixing process is as follows: adding polytetrafluoroethylene resin a and polytetrafluoroethylene resin b into a double-cone mixer, rotating clockwise for 10min and then rotating anticlockwise for 10min, wherein the mixing temperature is 10 ℃; the biaxial stretching process comprises the following steps: firstly, longitudinal stretching with the stretching ratio of 3 times is carried out, and then transverse stretching with the stretching ratio of 5 times is carried out; the curing temperature was 60 ℃.
Mixing raw materials 1.
Example 2:
a preparation method of polytetrafluoroethylene comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxially stretching, and further comprising a step of heat setting after biaxially stretching, wherein the heat setting temperature is 340 ℃, the heat setting time is 60s, and the cooling rate of the heat setting is 70 ℃/min; wherein, the material mixing process is as follows: adding polytetrafluoroethylene resin a and polytetrafluoroethylene resin b into a double-cone mixer, rotating clockwise for 30min, standing for 5min, and then rotating counterclockwise for 30min, wherein the mixing temperature is 20 ℃; the biaxial stretching process comprises the following steps: firstly, longitudinal stretching with the stretching ratio of 10 times is carried out, and then transverse stretching with the stretching ratio of 12 times is carried out; the curing temperature was 90 ℃.
Mixing the raw materials 2.
Example 3:
a preparation method of polytetrafluoroethylene comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxially stretching, and further comprising a step of heat setting after biaxially stretching, wherein the heat setting temperature is 330 ℃, the heat setting time is 50s, and the cooling rate of the heat setting is 50 ℃/min; wherein, the material mixing process is as follows: adding polytetrafluoroethylene resin a and polytetrafluoroethylene resin b into a double-cone mixer, rotating clockwise for 20min, standing for 3min, and then rotating counterclockwise for 20min, wherein the mixing temperature is 15 ℃; the biaxial stretching process comprises the following steps: firstly, performing longitudinal stretching with the stretching ratio of 5 times, and then performing transverse stretching with the stretching ratio of 8 times; the curing temperature is 80 ℃.
Mixing the raw materials 3.
Example 4:
a preparation method of polytetrafluoroethylene comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxially stretching, and further comprising a step of heat setting after biaxially stretching, wherein the heat setting temperature is 320 ℃, the heat setting time is 60s, and the cooling rate of the heat setting is 40 ℃/min; wherein, the material mixing process is as follows: adding polytetrafluoroethylene resin a and polytetrafluoroethylene resin b into a double-cone mixer, rotating clockwise for 25min, standing for 2min, and then rotating counterclockwise for 25min, wherein the mixing temperature is 15 ℃; the biaxial stretching process comprises the following steps: firstly, longitudinal stretching with the stretching ratio of 7 times is carried out, and then transverse stretching with the stretching ratio of 8 times is carried out; the curing temperature was 70 ℃.
Mixing the raw materials 4.
Example 5:
a preparation method of polytetrafluoroethylene comprises the following steps: mixing materials, curing, compacting, pushing, rolling and biaxially stretching, and further comprising a step of heat setting after biaxially stretching, wherein the heat setting temperature is 340 ℃, the heat setting time is 30s, and the cooling rate of the heat setting is 30 ℃/min; wherein, the material mixing process is as follows: adding polytetrafluoroethylene resin a and polytetrafluoroethylene resin b into a double-cone mixer, rotating clockwise for 30min, standing for 5min, and then rotating counterclockwise for 30min, wherein the mixing temperature is 20 ℃; the biaxial stretching process comprises the following steps: firstly, performing longitudinal stretching with the stretching ratio of 5 times, and then performing transverse stretching with the stretching ratio of 10 times; the curing temperature was 60 ℃.
Mixing raw materials 5.
Examples 1-5 were tested according to QB/T5002-2016, and the data shown in the following table were obtained:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A polytetrafluoroethylene bubble point membrane is characterized in that: the raw material is polytetrafluoroethylene resin with a molecular weight of 105-107And the molecular weight of the polytetrafluoroethylene resin a is 107-108The polytetrafluoroethylene resin b, the polytetrafluoroethylene resin a and polytetrafluoroethyleneThe average particle diameter ratio of the vinyl resin b is 95-105: 100, the weight ratio of the polytetrafluoroethylene resin a to the polytetrafluoroethylene resin b is (1-6): 20.
2. a polytetrafluoroethylene bubble point membrane according to claim 1, wherein: the pore diameter of the bubble point membrane is 0.1-0.3 micron, and the porosity is 85-95%.
3. A method of making the polytetrafluoroethylene bubble point membrane of claim 1 comprising the steps of: compounding, curing, pressed compact, bulldoze, calendering and biaxial stretching, its characterized in that: the method also comprises a heat setting step after biaxial stretching, wherein the heat setting temperature in the heat setting step is 320-340 ℃, and the heat setting time is 30-60 s.
4. The method for preparing a polytetrafluoroethylene bubble point membrane according to claim 3, wherein the method comprises the following steps: the mixing temperature is 10-20 ℃; the curing temperature is 60-90 ℃.
5. The method for preparing a polytetrafluoroethylene bubble point membrane according to claim 3, wherein the method comprises the following steps: the cooling rate of the heat setting is 20-70 ℃/min.
6. The method for preparing a polytetrafluoroethylene bubble point membrane according to claim 3, wherein the method comprises the following steps: the bidirectional stretching process comprises the steps of firstly performing longitudinal stretching with the stretching ratio of 3-10 times, and then performing transverse stretching with the stretching ratio of 5-12 times.
7. The method for preparing a polytetrafluoroethylene bubble point membrane according to claim 3, wherein the method comprises the following steps: and during material mixing, a double-cone mixer is adopted for material mixing, and during material mixing, the double-cone mixer rotates clockwise for 10-30min, stands for 0-5min and then rotates anticlockwise for 10-30 min.
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Denomination of invention: A polytetrafluoroethylene bubble point film and its preparation method Effective date of registration: 20220622 Granted publication date: 20211015 Pledgee: South Taihu New Area sub branch of Huzhou Wuxing Rural Commercial Bank Co.,Ltd. Pledgor: ZHEJIANG KERTICE HI-TECH FLUOR-MATERIAL CO.,LTD. Registration number: Y2022980008396 |
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Date of cancellation: 20230731 Granted publication date: 20211015 Pledgee: South Taihu New Area sub branch of Huzhou Wuxing Rural Commercial Bank Co.,Ltd. Pledgor: ZHEJIANG KERTICE HI-TECH FLUOR-MATERIAL CO.,LTD. Registration number: Y2022980008396 |